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WO1992007103A1 - Appareil et procede de depot en phase gazeuse - Google Patents

Appareil et procede de depot en phase gazeuse Download PDF

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Publication number
WO1992007103A1
WO1992007103A1 PCT/GB1991/001771 GB9101771W WO9207103A1 WO 1992007103 A1 WO1992007103 A1 WO 1992007103A1 GB 9101771 W GB9101771 W GB 9101771W WO 9207103 A1 WO9207103 A1 WO 9207103A1
Authority
WO
WIPO (PCT)
Prior art keywords
evaporation crucible
vapour
evaporation
charge
crucible
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/GB1991/001771
Other languages
English (en)
Inventor
Alan William Bishop
David John Bray
Robert William Gardiner
Brian William Viney
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
UK Secretary of State for Defence
Original Assignee
UK Secretary of State for Defence
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by UK Secretary of State for Defence filed Critical UK Secretary of State for Defence
Priority to JP51647291A priority Critical patent/JP3475403B2/ja
Priority to US08/039,409 priority patent/US5348703A/en
Priority to EP91919320A priority patent/EP0553228B1/fr
Priority to DE69105992T priority patent/DE69105992T2/de
Priority to CA002094132A priority patent/CA2094132C/fr
Publication of WO1992007103A1 publication Critical patent/WO1992007103A1/fr
Priority to GB9306947A priority patent/GB2264952B/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/243—Crucibles for source material

Definitions

  • the present invention relates to an improved apparatus and method for the production of alloys by a physical vapour deposition process generally as described in our earlier British Patents GB 1206586 and GB 126595>
  • the apparatus is operated under vacuum within a vacuum chamber and the alloy constituents are evaporated from one or more evaporation baths before being caused to condense upon a temperature-controlled collector.
  • the apparatus and method described here are suitable for producing alloys in substantial quantities and with sufficient structural integrity that the deposits may be removed from the collector intact.
  • the deposit can then be worked into sheet, strip or other wrought form and heat-treated to achieve the desired mechanical properties.
  • the deposited alloy may be heat- treated before, during or after working.
  • the deposited alloy may be removed and pulverised for subsequent powder metallurgical techniques, for example when it is desired to produce an article close in form to the intended final shape.
  • magnesium alloys have yet to find widespread use in aerospace applications, partly because of certain shortcomings in their mechanical properties, but principally because of their poor corrosion resistance.
  • RSR rapid solidification rate
  • elements such as aluminium, chromium or silicon
  • This inefficacy is due to their poor solubilities in the magnesium matrix: Under normal equilibrium conditions the concentration of such additives in solid solution is too low to provide an effective barrier to corrosion.
  • Rapid solidification techniques including vapour deposition provide the means to overcome equilibrium thermodynamic constraints and achieve compositions which are beyond the scope of the ingot metallurgist by "freezing" constituent atoms in position before they have the opportunity to migrate and segregate as they would in conventional ingot processes. These techniques therefore offer a possible route to improved corrosion resistance in magnesium alloys by allowing an increase in the population of corrosion-inhibiting species in the magnesium alloy without forming harmful precipitates.
  • Physical vapour deposition is favoured over other forms of RSR processing for a number of reasons. Firstly, the cooling rate is very much higher in physical vapour deposition and thereby increases the likelihood of formation of solid solutions. Secondly, physical vapour deposition offers a considerable choice of potential alloying constituents since the candidate elements are raised to the vapour state, thereby ensuring miscibility between different constituents. By contrast, other forms of RSR processing are limited in the possible combinations of alloying constituents which they can offer to those elements which are miscible in the molten state. This is a particularly important consideration in the case of magnesium since, at the melting temperature of many potentially interesting alloying additions, magnesium has a very high vapour pressure and hence evaporates very quickly.
  • Another way of minimising non-uniformity is to introduce lateral movement between the relative positions of the collector and the sources. In practice it is easier to keep the sources stationary and to move the collector, either by rotation or by a reciprocating motion, thereby ensuring that exposure of different parts of the substrate to the respective sources is equalised. Whilst a moving collector offers considerable benefit in improving the homogeneity of the deposit, a small degree of non-uniformity is inevitable because the deposit is effectively laid down as a series of sub-layers which are alternately rich in one particular constituent. In a structural member even this level of non-uniformity could be critical to its overall strength and might also be bad from the point of view of corrosion resistance.
  • the invention is an apparatus for the production of an alloy by a process of evaporating the alloy constituents under vacuum and condensing the constituent vapours on a collector, the apparatus comprising two heated evaporation crucibles, heating control means for independently regulating the temperatures of charges in the evaporation crucibles at the desired levels to maintain appreciable vapour pressures and generate rising streams of vapour from the respective charges, and a temperature-controlled collector positioned such that it captures the vapours emitted from the evaporation crucibles, characterised by the following features in combination:
  • an electron beam heater to heat the charge in the first evaporation crucible
  • radiant heating means to heat the charge in the second evaporation crucible
  • a closure for the second evaporation crucible which closure is equipped with an array of nozzles spaced around a collector-facing surface thereof, the nozzles being oriented to direct the streams of vapour from the second evaporation crucible along convergent pathways which intersect the vapour stream emitted from the first evaporation crucible to facilitate mixing between the respective vapour streams before they are captured by the collector.
  • the invention provides a method of producing an alloy by a process of evaporating the alloy constituents under vacuum and condensing the constituent vapours on a collector, the method comprising evaporating a charge of a first alloy constituent or constituents from a first evaporation crucible, allowing the vapour flux from the first evaporation crucible to rise towards the collector, evaporating a charge of a further alloy constituent or constituents from a second evaporation crucible, and maintaining the flow of constituent vapours from the respective evaporation crucibles by continued heating of the charges in order to ensure that the vapour which is captured by the collector is made up of vapours from the first and second evaporation crucibles, characterised by the following steps in combination:
  • vapour from the second evaporation crucible in streams through a series of convergently-directed nozzles arranged in an array around the first evaporation crucible such that these streams are caused to flow towards the collector along pathways which intersect the rising vapour flux from the first evaporation crucible to facilitate mixing between the respective vapours before they are captured by the collector.
  • the invention provides a method of producing an alloy by a process of evaporating the alloy constituents under vacuum and condensing the constituent vapours on a collector, the method comprising evaporating a charge of a first alloy constituent or constituents from a first evaporation crucible, allowing the vapour flux from the first evaporation crucible to rise towards the collector, evaporating a charge of a further alloy constituent or constituents from a second evaporation crucible, and maintaining the flow of constituent vapours from the respective evaporation crucibles by continued heating of the charges in order to ensure that the vapour which is captured by the collector is made up of vapours from the first and second evaporation crucibles, characterised by the following steps in combination:
  • the closure or lid in which they are located is preferably heated independently from the body of the second evaporation crucible to a temperature which is higher than the crucible temperature.
  • the nozzles are of re-entrant form so that the major part of the nozzle body is located within the crucible, thereby minimising the effects of cooling.
  • the surface of the crucible lid between the nozzles may be coated with a ceramic paste which serves as an insulating layer.
  • the vapour pressure of magnesium is very high so the dimensions of the nozzles must be chosen such that the desired flow rate of magnesium vapour from the second evaporation crucible is obtainable by regulating the temperature of the crucible above this oxide dispersion temperature.
  • the deposition rate is regulated to between 2 and 4 mm per hour, although it is possible to increase this rate to 6mm per hour or even greater.
  • One of the drawbacks of higher deposition rates is that there is an increased tendency for the deposit to exhibit porosity so in practice the deposition rate is optimised to achieve a sensible microstructure.
  • porosity can be largely eliminated by mechanically working the deposit at intervals during its deposition in order to flatten surface asperities. In a moving collector apparatus, such mechanical working is preferably carried out after each pass of the collector over the evaporation sources. This ensures that the vapour stream always impinges on a flat surface which is free from columnar growth.
  • Figure 1 is a schematic diagram showing a general layout for the apparatus of the invention
  • Figure 2 is a plan view of a preferred form of the apparatus.
  • Figure 3 is a sectional view on line XX' of Figure 2.
  • FIG. 1 there is shown an inner evaporation crucible 1 surrounded by a second evaporation crucible 2.
  • the inner evaporation crucible 1 contains a charge 3 of a relatively low volatility constituent whilst second evaporation crucible 2 is charged with a much higher volatility constituent 4, such as magnesium.
  • the crucibles are centrally positioned under a collector 5 on which a deposit 6 is accumulated.
  • the charge 3 in the inner evaporation crucible 1 is heated using an electron beam 7 focussed by magnet 8 to a temperature which causes a stream of vapour to rise towards collector 5.
  • Second evaporation crucible 2 is heated by radiant heaters (not shown) to generate an appreciable vapour pressure in the magnesium 4, such that streams of magnesium vapour are discharged towards the collector through nozzles 9-
  • the nozzles 9 are angled towards the collector so that the streams of magnesium vapour intersect the stream of vapour rising from the inner evaporation crucible 1. This ensures that the combined vapour impinging on the collector 5 is an intimate mixture of constituents.
  • Each stream of magnesium vapour diverges after it leaves its respective nozzle 9 so the spacing between individual nozzles and their separation from the collector 5 is arranged such that a uniform population of magnesium atoms is delivered to the collector across a large proportion of its total surface area.
  • the separation between the inner evaporation crucible 1 and the collector is also chosen to give uniform coverage over as much of the collector as possible.
  • FIGs 2 and 3 show a preferred form of the apparatus in plan view and sectional view, respectively.
  • the inner evaporation crucible 10 is shown as a water-cooled copper crucible which is surrounded by an annular steel crucible 20.
  • Annular steel crucible 20 is covered with a steel lid 21 having eight nozzles 4 ⁇ disposed around its inner circumference, which nozzles are convergently directed towards a collector (not shown) positioned above the inner crucible 10.
  • the nozzles 40 are of re-entrant form, having their bodies protruding into the chamber defined by the annular steel crucible 20 and its id 21, thereby ensuring that heat losses through the nozzles are kept to a minimum.
  • Annular steel crucible 20 is itself surrounded by an arrangement of four ceramic bricks 24, 25, 26 and 27 which are fastened together by retaining clips 28. These bricks then form a complete ring serving as a support for radiant heater 30 which is housed in grooves 29 formed on the interior faces of the ceramic bricks.
  • the steel lid 21 is similarly covered by a ceramic ring 31 which has grooves 32 formed bn its tinderside for retention of a second radiant heater 33•
  • Radiant heaters 3 and 33 may be formed from an iron/aluminium alloy such as Kanthai S (Registered Trade Hark) or from tantalum.
  • Kanthai S Registered Trade Hark
  • these radiant heaters are preferably configured in the form of return loops. This ensures that the large currents carried by the heating elements during operation of the apparatus do not generate biassing magnetic fields.
  • Thermocouples 34 are attached to the base of the annular steel crucible 20 to monitor its temperature, and to minimise thermal conduction away from the annular steel crucible 20 by the coolant water circulating around inner evaporation crucible 10 a pack of thermally insulating screens 35 s inserted between the crucibles. Further screens (not shown) may also be placed over the top of the top surface of the water-cooled crucible as an additional measure to minimise thermal conduction away from the annular steel crucible 20. Depending on the particular constituents to be evaporated, and consequently the temperature differences expected between the crucibles, screens 35 may be formed from molybdenum, stainless steel or possibly ceramic fibre materials.
  • a charge of magnesium metal is placed in annular steel crucible 20 and the temperature of the crucible is then raised to between 700 and 800 ⁇ C using the radiant heater 30.
  • Radiant heater 33 is independently controlled to heat the steel lid 21 to a temperature which is greater than that of the crucible by at least 50°C, but preferably by about 100°C, to reduce the risk to nozzles 40 of blockage by undesired condensation of magnesium vapour.
  • the surface of the magnesium is free of oxide film and an appreciable vapour pressure of magnesium builds up inside the crucible.
  • the escape of magnesium vapour from the crucible is attenuated by the nozzles 40 which are dimensioned to give a satisfactory flow rate for effective performance of the deposition process.
  • the inner evaporation crucible 10 is loaded with a charge of the desired transition metal element or elements and the surface of this charge is bombarded with an electron beam to effect evaporation.
  • the water cooled copper crucible shown here in Figures 2 and 3 is universally applicable for the evaporation of all potential alloying additions but suffers from the drawback that it conducts heat away from the evaporation surface and is therefore inefficient in its use of energy.
  • Some alloying additions can be evaporated from graphite or ceramic crucibles, provided that chemical reaction between the crucible material and the alloying addition is not too severe.
  • a shutter (not shown) is used to screen the collector from the evaporation sources until an equilibrium condition is reached where steady flow rates of the magnesium and constituent vapours are achieved. The shutter is then opened and the collector is exposed to the vapour mixture until the deposit has reached the required thickness, at which point the shutter is closed again. The radiant heaters and electron beam are turned off and the deposit is allowed to cool before removal from the collector for further processing.
  • the central crucible can be configured as a water-cooled annulus which is fed by an alloy rod in accordance with known techniques. This imparts greater flexibility to the apparatus as it allows semi-continuous deposition rather than the batch deposition which results from using a single charge in a conventional crucible.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Electroluminescent Light Sources (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Un appareil de dépôt physique en phase gazeuse d'un alliage, dont les éléments constitutifs présentent des pressions de vapeur très différentes, comprend un creuset d'évaporation interne (1) entouré par un second creuset d'évaporation (2) pourvu d'un alignement de tuyères (9) orientées vers un collecteur (5). Lors de l'utilisation de l'appareil, une charge (3) de volatilité relativement faible est évaporée dans le creuset interne (1) par l'intermédiaire d'un faisceau d'électrons (7) focalisé par un aimant (8). La charge (4) se trouvant dans le second creuset (2) présente une volatilité beaucoup plus élevée et est évaporée par chauffage rayonnant. Les tuyères (9) dirigent la vapeur provenant de la charge (4) le long de trajectoires qui entrecoupent la vapeur s'élevant de la charge (3) de sorte que le flux de vapeurs combinées parvenant au collecteur (5) est un mélange étroit de constituants. Les tuyères (9) peuvent aussi être utilisées pour réguler la vitesse d'écoulement de la vapeur provenant du second creuset (2).
PCT/GB1991/001771 1990-10-16 1991-10-11 Appareil et procede de depot en phase gazeuse Ceased WO1992007103A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
JP51647291A JP3475403B2 (ja) 1990-10-16 1991-10-11 蒸着装置及び蒸着方法
US08/039,409 US5348703A (en) 1990-10-16 1991-10-11 Vapor deposition apparatus and method
EP91919320A EP0553228B1 (fr) 1990-10-16 1991-10-11 Appareil et procede de depot en phase gazeuse
DE69105992T DE69105992T2 (de) 1990-10-16 1991-10-11 Vorrichtung und verfahren zum aufdampfen.
CA002094132A CA2094132C (fr) 1990-10-16 1991-10-11 Methode et dispositif de deposition en phase vapeur
GB9306947A GB2264952B (en) 1990-10-16 1993-04-02 Vapour deposition apparatus and method

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9022449.4 1990-10-16
GB9022449A GB2248852A (en) 1990-10-16 1990-10-16 Vapour deposition

Publications (1)

Publication Number Publication Date
WO1992007103A1 true WO1992007103A1 (fr) 1992-04-30

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1991/001771 Ceased WO1992007103A1 (fr) 1990-10-16 1991-10-11 Appareil et procede de depot en phase gazeuse

Country Status (8)

Country Link
US (1) US5348703A (fr)
EP (1) EP0553228B1 (fr)
JP (1) JP3475403B2 (fr)
AT (1) ATE115646T1 (fr)
CA (1) CA2094132C (fr)
DE (1) DE69105992T2 (fr)
GB (2) GB2248852A (fr)
WO (1) WO1992007103A1 (fr)

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AU2001247779A1 (en) 2000-03-24 2001-10-08 Cymbet Corporation Low-temperature fabrication of thin-film energy-storage devices
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US7603144B2 (en) 2003-01-02 2009-10-13 Cymbet Corporation Active wireless tagging system on peel and stick substrate
US7294209B2 (en) 2003-01-02 2007-11-13 Cymbet Corporation Apparatus and method for depositing material onto a substrate using a roll-to-roll mask
US6906436B2 (en) * 2003-01-02 2005-06-14 Cymbet Corporation Solid state activity-activated battery device and method
DE10341914B4 (de) * 2003-09-11 2008-08-14 Forschungszentrum Karlsruhe Gmbh Einrichtung zur Herstellung dünner Schichten und Verfahren zum Betreiben der Einrichtung
US7211351B2 (en) 2003-10-16 2007-05-01 Cymbet Corporation Lithium/air batteries with LiPON as separator and protective barrier and method
EP1714333A2 (fr) 2004-01-06 2006-10-25 Cymbet Corporation Structure barriere en couches possedant une ou plusieurs couches definissables et procede
US7776478B2 (en) 2005-07-15 2010-08-17 Cymbet Corporation Thin-film batteries with polymer and LiPON electrolyte layers and method
JP2009502011A (ja) 2005-07-15 2009-01-22 シンベット・コーポレイション 軟質および硬質電解質層付き薄膜電池および方法
US20070098880A1 (en) * 2005-10-28 2007-05-03 Jean-Pierre Tahon Method of vaporization of phosphor precursor raw materials
US20090162535A1 (en) * 2007-12-21 2009-06-25 Jean-Pierre Tahon Method of forming a phosphor or scintillator material and vapor deposition apparatus used therefor
JP5677785B2 (ja) * 2009-08-27 2015-02-25 三星ディスプレイ株式會社Ｓａｍｓｕｎｇ Ｄｉｓｐｌａｙ Ｃｏ．，Ｌｔｄ． 薄膜蒸着装置及びこれを利用した有機発光表示装置の製造方法
US10601074B2 (en) 2011-06-29 2020-03-24 Space Charge, LLC Rugged, gel-free, lithium-free, high energy density solid-state electrochemical energy storage devices
US11996517B2 (en) 2011-06-29 2024-05-28 Space Charge, LLC Electrochemical energy storage devices
US9853325B2 (en) 2011-06-29 2017-12-26 Space Charge, LLC Rugged, gel-free, lithium-free, high energy density solid-state electrochemical energy storage devices
US11527774B2 (en) 2011-06-29 2022-12-13 Space Charge, LLC Electrochemical energy storage devices
KR20130004830A (ko) 2011-07-04 2013-01-14 삼성디스플레이 주식회사 유기층 증착 장치 및 이를 이용한 유기 발광 표시 장치의 제조 방법
US20160281212A1 (en) 2015-03-24 2016-09-29 Siva Power, Inc. Thermal management of evaporation sources
CN107012432B (zh) * 2017-05-08 2019-01-18 京东方科技集团股份有限公司 一种蒸发源及蒸镀装置
WO2019173626A1 (fr) 2018-03-07 2019-09-12 Space Charge, LLC Dispositifs d'accumulation d'énergie à électrolyte solide à film mince
CN112553579B (zh) * 2019-09-26 2023-05-09 宝山钢铁股份有限公司 一种具有过滤及均匀化喷嘴的真空镀膜装置

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Also Published As

Publication number Publication date
GB2264952A (en) 1993-09-15
CA2094132C (fr) 2001-07-10
GB9306947D0 (en) 1993-06-02
GB9022449D0 (en) 1990-11-28
EP0553228B1 (fr) 1994-12-14
JP3475403B2 (ja) 2003-12-08
DE69105992D1 (de) 1995-01-26
CA2094132A1 (fr) 1992-04-17
JPH06501989A (ja) 1994-03-03
US5348703A (en) 1994-09-20
DE69105992T2 (de) 1995-05-04
GB2248852A (en) 1992-04-22
GB2264952B (en) 1994-04-20
EP0553228A1 (fr) 1993-08-04
ATE115646T1 (de) 1994-12-15

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